CN113862619B - Zinc-magnesium target material and preparation method thereof - Google Patents
Zinc-magnesium target material and preparation method thereof Download PDFInfo
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- CN113862619B CN113862619B CN202111050306.4A CN202111050306A CN113862619B CN 113862619 B CN113862619 B CN 113862619B CN 202111050306 A CN202111050306 A CN 202111050306A CN 113862619 B CN113862619 B CN 113862619B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to the technical field of targets, and discloses a zinc-magnesium target and a preparation method thereof, wherein the preparation method comprises the following steps: putting the simple substance zinc and the simple substance magnesium into a vacuum smelting furnace for smelting, fully stirring and preserving heat after smelting to obtain mixed smelting liquid; pouring the mixed smelting liquid to form zinc-magnesium alloy pressed material; heating the zinc-magnesium alloy pressing material, and extruding through a first die after heating to obtain a first extrusion material; extruding by adopting a second die, a third die and a N die in sequence to obtain a target blank; and machining the target blank to obtain the zinc-magnesium target. The zinc-magnesium target material manufactured by the preparation method has the advantages of high internal object defect, high density and average grain size smaller than 200 microns, and the zinc-magnesium target material is adopted for sputtering, so that uniform and fine grains are not only conducive to obtaining a thin film functional layer with uniform film thickness, but also can avoid discharge and ignition phenomena in the sputtering process.
Description
Technical Field
The invention relates to the technical field of targets, in particular to a zinc-magnesium target and a preparation method thereof.
Background
The zinc-magnesium target is applied to the field of solar thin film batteries, oxygen and metal ions sputtered by the zinc-magnesium target are introduced in the magnetron sputtering process to form zinc-magnesium oxide and deposit the zinc-magnesium oxide on the photovoltaic glass. However, in practical application, because the smelting temperature of the zinc oxide magnesium target material is up to 2000 ℃, the zinc oxide magnesium target material can only be prepared by adopting a powder metallurgy mode. The powder metallurgy target material of the type has defects in the general interior, has low density of only 92 percent, is easy to generate abnormal discharge phenomenon in the sputtering process, and causes uneven thickness of a film correspondingly deposited on the panel.
Disclosure of Invention
In order to solve the technical problems, the invention provides the zinc-magnesium target and the preparation method thereof, which ensure that the inside of the target is free from defects, improve the compactness of the zinc-magnesium target and avoid discharge phenomenon in the sputtering process.
The technical scheme adopted for solving the technical problems is as follows:
the preparation method of the zinc-magnesium target comprises the following steps:
(1) Putting the simple substance zinc and the simple substance magnesium into a vacuum smelting furnace for smelting, fully stirring and preserving heat after smelting to obtain mixed smelting liquid;
(2) Pouring the mixed smelting liquid to form zinc-magnesium alloy pressed material;
(3) Heating the zinc-magnesium alloy pressing material, and extruding through a first die after heating to obtain a first extrusion material;
(4) Extruding by adopting a second die, a third die and a N die in sequence to obtain a target blank;
(5) And machining the target blank to obtain the zinc-magnesium target.
Preferably, in the step (1), the smelting temperature is 550+/-10 ℃ and the heating rate is 20 ℃ per minute, and the vacuum degree of the smelting furnace is less than 0.01Pa.
Preferably, in the step (1), the incubation time is 15 minutes.
Preferably, in the step (3) or (4), the pressing heads are used for pressing, the dies each comprise a die body, an extrusion cavity is formed in the die body, and an extrusion rod is coaxially arranged in the extrusion cavity.
Preferably, in the step (3) or (4), the deformation amount of the extrusion material at each extrusion is 3 to 5 mm.
Preferably, in the step (3) or (4), the die is kept at 300 ℃ for 25-35 minutes during the extrusion process.
Preferably, in the step (3) or (4), the extruded material is heated to 370-385 ℃ before extrusion.
Preferably, the target blank is annealed at 340-350 ℃ for 2.5-3 hours before machining.
Preferably, in the step (5), machining is performed at 525-625 RPM and 0.08-0.12 mm/pass of the inner diameter, outer diameter and length of the target blank until the target outer scale is completely removed and the required dimensional tolerance is achieved.
A zinc-magnesium target material is prepared by the preparation method of the zinc-magnesium target material.
Compared with the prior art, the beneficial effects of the method are as follows: the zinc-magnesium target material manufactured by the preparation method has the advantages of high internal object defect, high density and average grain size smaller than 200 microns, and the zinc-magnesium target material is adopted for sputtering, so that uniform and fine grains are not only conducive to obtaining a thin film functional layer with uniform film thickness, but also can avoid discharge and ignition phenomena in the sputtering process.
Drawings
FIG. 1 is a schematic illustration of extrusion of an extrusion material of the present invention.
Wherein: 1-pressure head, 2-zinc magnesium alloy pressing, 3-first die, 31-die body, 32-extrusion rod, 4-N die, 5-target blank and 100-air hole defect.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples. The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
The zinc-magnesium target material of the preferred embodiment of the invention has the magnesium content of 1-10 percent and is prepared by the following preparation method:
(1) And (3) putting the elemental zinc and the elemental magnesium into a vacuum smelting furnace for smelting, fully stirring and preserving heat after smelting to obtain a mixed smelting liquid. Wherein the smelting temperature is 550+/-10 ℃, the heating rate is 20 ℃ per minute, the vacuum degree of the smelting furnace is less than 0.01Pa, and the heat preservation time is 15 minutes.
Further, since magnesium is very reactive and causes spontaneous combustion by static electricity in air, and the melting point of magnesium is 651 degrees celsius and the melting point of zinc is 419 degrees celsius, an alumina crucible is required for melting.
(2) And pouring the mixed smelting liquid to form the zinc-magnesium alloy pressing material 2. When in pouring, a die is adopted for direct pouring, the obtained zinc-magnesium alloy pressing material is hollow and cylindrical, and the inside of the zinc-magnesium alloy pressing material generally contains 3-5 mm air hole defects 100, and the number of the air hole defects is within 10.
(3) And heating the zinc-magnesium alloy pressing material 2 to 370-385 ℃, preferably 380 ℃, and extruding through a first die 3 after heating to obtain a first extrusion material. Referring to fig. 1, the extrusion is performed by using a pressing head 1, meanwhile, the die comprises a die body 31, an extrusion cavity is formed in the die body 31, an extrusion rod 32 is coaxially arranged in the extrusion cavity, the extrusion rod 32 comprises an extrusion part and a guiding part, the guiding part is close to the pressing head 1, and the diameter of the guiding part gradually decreases towards the direction close to the pressing head 1, so that the zinc magnesium alloy pressing material 2 is conveniently sleeved in the extrusion cavity for extrusion. The extrusion cavity can be a cavity or a groove, and correspondingly extruded extrusion materials can be taken out from the front end of the extrusion cavity or the rear end of the extrusion cavity.
In addition, the die is required to be kept at 300 ℃ for 25-35 minutes, preferably 30 minutes, in the extrusion process, so that adhesion or stress release cold cracking caused by overlarge temperature difference between the zinc-magnesium alloy pressing material and the die is prevented.
(4) Extruding by adopting a second die, a third die and a N die 4 in sequence to obtain a target blank 5; the operation mode of the step (3) is the same as that of the step (3), and the adopted die is different in size. Specifically, the inner diameter of the extrusion cavity and the outer diameter of the extrusion rod 32 of the first die, the second die, the third die and the N die 5 are all different, so that the size of the extruded material is gradually changed to the target size after multiple times of extrusion, and meanwhile, the internal air hole defects 100 of the extruded material gradually disappear, and finally, the target blank is obtained.
In addition, in the step (3) or (4), the deformation amount of the extruded material at each extrusion is 3 to 5 mm. This is summarized by repeated experiments, and too large deformation will lead to extrusion cracking of the extrusion; if the deformation amount is too small, the function of closing internal defects is lost, and finally, the high-purity zinc-magnesium cylinder with no defect in the material and excellent performance can not be obtained.
(5) And machining the target blank 5 to obtain the zinc-magnesium target. The target blank 5 is annealed at 340-350 c, preferably 350 c, for 2.5-3 hours, preferably 3 hours, before machining. And machining, namely machining the inner diameter, the outer diameter and the length of the target blank at 525-625 RPM and 0.08-0.12 mm/channel of feed amount until the outer oxide skin of the target is completely removed and reaches the required dimensional tolerance, and finally binding the target blank with a back pipe.
The zinc-magnesium target material manufactured by the preparation method has the advantages of high internal object defect, high density and average grain size smaller than 200 microns, and the zinc-magnesium target material is adopted for sputtering, so that uniform and fine grains are not only conducive to obtaining a thin film functional layer with uniform film thickness, but also can avoid the ignition phenomenon of a discharge machine in the sputtering process.
In addition, the preparation method can effectively improve the material utilization rate. The weight ratio of traditional cast ingot feeding and finished product is 1.8:1, namely, 1.8Kg of finished target material can be prepared. The invention can effectively reduce the feeding ratio to 1.2-1.1.25: 1, the material utilization rate is increased, and the cost is reduced.
Meanwhile, the extrusion mode used by the invention is different from the traditional hot extrusion machine, the hot extrusion machine requires 2 tons of feeding, and the 500 tons of investment of one hot extrusion device exceeds 800 ten thousand, and the investment cost of the matched extrusion die of the extrusion machine used in the invention is within 100 ten thousand.
The material prepared by the preparation method is suitable for preparing zinc-magnesium alloy with the magnesium content of 1-10%, and a corresponding sputtering film layer is not required to be obtained by synthesizing a zinc-magnesium oxide target at a high temperature of over 2000 ℃.
For a better understanding of the present invention, some specific examples are provided herein:
example 1
The zinc-magnesium target is prepared by the following preparation method, which comprises the following steps:
(1) Putting the elemental zinc and the elemental magnesium into a vacuum smelting furnace with the vacuum degree of less than 0.01Pa for smelting, wherein the smelting temperature is 550 ℃, and fully stirring and preserving heat for 15 minutes after smelting;
(2) Casting the mixed smelting into a die with the outer diameter of 180 and the inner diameter of 80mm and the length of 400 to form a hollow zinc-magnesium alloy pressing material;
(3) And (3) heating the whole zinc-magnesium alloy pressing material 2 to 370 ℃, and passing through a first die 3 under the action of a pressing head 1 to obtain a first pressing material with the outer diameter of 170mm and the inner diameter of 90 mm. Wherein, the first die 3 is insulated at 300 ℃ for 25 minutes in the extrusion process.
(4) And after extrusion is finished, reheating the first extrusion material to 370 ℃, and preserving heat for 25min. And extruding by adopting a second die, and repeating the steps until the extruded material is extruded to a target blank 5 with the outer diameter of 163mm and the inner diameter of 130 mm.
In the extrusion process, the length of the zinc-magnesium alloy pressing material 2 is prolonged, crystal grains are synchronously refined, defects such as internal air holes in the material are closed, and the density is improved to 99.2%.
(5) And (3) annealing the target blank 5 at 340 ℃ for 2.5 hours, and machining the target blank 5 at 525RPM (revolutions per minute) with a feed of 0.08 mm/channel to obtain the zinc-magnesium target.
The obtained zinc-magnesium target material is detected, the interior of the zinc-magnesium target material is defect-free, the density is high, the average grain size is 191 microns, the film thickness is uniform when sputtering is carried out, and the phenomena of discharge and ignition are avoided.
Example two
The zinc-magnesium target is prepared by the following preparation method, which comprises the following steps:
(1) Putting the elemental zinc and the elemental magnesium into a vacuum smelting furnace with the vacuum degree of less than 0.01Pa for smelting, wherein the smelting temperature is 560 ℃, and fully stirring and preserving heat for 15 minutes after smelting;
(2) Casting the mixed smelting into a die with the outer diameter of 180 and the inner diameter of 80mm and the length of 400 to form a hollow zinc-magnesium alloy pressing material;
(3) And (3) heating the whole zinc-magnesium alloy pressing material 2 to 380 ℃, and passing through a first die 3 under the action of a pressing head 1 to obtain a first pressing material with the outer diameter of 170mm and the inner diameter of 90 mm. Wherein, the first die 3 is insulated at 300 ℃ for 30 minutes in the extrusion process.
(4) And after extrusion is finished, reheating the first extrusion material to 380 ℃, and preserving heat for 30min. And extruding by adopting a second die, and repeating the steps until the extruded material is extruded to a target blank 5 with the outer diameter of 163mm and the inner diameter of 130 mm.
In the extrusion process, the length of the zinc-magnesium alloy pressing material 2 is prolonged, crystal grains are synchronously refined, defects such as internal air holes in the material are closed, and the density is improved to 99.5%.
(5) And (3) annealing the target blank 5 at 350 ℃ for 3 hours, and machining the target blank 5 at 525RPM (revolutions per minute) at a feed rate of 0.1 mm/channel to obtain the zinc-magnesium target.
The obtained zinc-magnesium target material is detected, the interior of the zinc-magnesium target material is defect-free, the density is high, the average grain size is 186 microns, the film thickness is uniform when sputtering is carried out, and the phenomena of discharge and ignition are avoided.
Example III
The zinc-magnesium target is prepared by the following preparation method, which comprises the following steps:
(1) Putting the elemental zinc and the elemental magnesium into a vacuum smelting furnace with the vacuum degree of less than 0.01Pa for smelting, wherein the smelting temperature is 555 ℃, and fully stirring and preserving heat for 15 minutes after smelting;
(2) Casting the mixed smelting into a die with the outer diameter of 180 and the inner diameter of 80mm and the length of 400 to form a hollow zinc-magnesium alloy pressing material;
(3) And (3) heating the whole zinc-magnesium alloy pressing material 2 to 385 ℃, and passing through a first die 3 under the action of a pressing head 1 to obtain a first pressing material with the outer diameter of 170mm and the inner diameter of 90 mm. Wherein, the first die 3 is insulated at 300 ℃ for 35 minutes in the extrusion process.
(4) And after the extrusion is finished, reheating the first extrusion material to 385 ℃, and preserving the heat for 35min. And extruding by adopting a second die, and repeating the steps until the extruded material is extruded to a target blank 5 with the outer diameter of 163mm and the inner diameter of 130 mm.
In the extrusion process, the length of the zinc-magnesium alloy pressing material 2 is prolonged, crystal grains are thinned synchronously, defects such as internal air holes in the material are closed, and the density is improved to 99.2.
(5) And (3) annealing the target blank 5 at 345 ℃ for 2.8 hours, and machining the target blank 5 at 525RPM (revolutions per minute) with a feed rate of 0.12 mm/channel to obtain the zinc-magnesium target.
The obtained zinc-magnesium target material is detected, the interior of the zinc-magnesium target material is defect-free, the density is high, the average grain size is 189 microns, and the film thickness is uniform and uniform when sputtering is carried out, so that the phenomena of discharge and ignition are avoided.
Comparative example one
This example differs from example one in that the heating temperature in steps (3), (4) is 400 ℃. The obtained zinc-magnesium target material has the partial melting phenomenon, the yield strength is not reduced, the quality of the zinc-magnesium target material is poor, and the requirement is not met.
Comparative example two
This example differs from example one in that the incubation temperature in steps (3) and (4) was 200℃and the incubation time was 20 minutes. The obtained zinc-magnesium target has local cracks, and the quality of the zinc-magnesium target is poor and does not meet the requirements.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and substitutions can be made by those skilled in the art without departing from the technical principles of the present invention, and these modifications and substitutions should also be considered as being within the scope of the present invention.
Claims (8)
1. A preparation method of a zinc-magnesium target material is characterized by comprising the following steps: the method comprises the following steps:
(1) Putting the simple substance zinc and the simple substance magnesium into a vacuum smelting furnace for smelting, fully stirring and preserving heat after smelting to obtain mixed smelting liquid;
(2) Pouring the mixed smelting liquid to form zinc-magnesium alloy pressed material;
(3) Heating the zinc-magnesium alloy pressing material, and extruding through a first die after heating to obtain a first extrusion material;
(4) Extruding by adopting a second die, a third die and a N die in sequence to obtain a target blank;
in the step (3) or (4), extrusion is performed by adopting a pressure head, wherein the dies comprise die bodies, extrusion cavities are arranged in the die bodies, extrusion rods are coaxially arranged in the extrusion cavities, and the inner diameters of the extrusion cavities and the outer diameters of the extrusion rods of the first die, the second die, the third die and the N die are different;
(5) And (3) machining the target blank to obtain the zinc-magnesium target, wherein the target blank is annealed at 340-350 ℃ for 2.5-3 hours before machining.
2. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (1), the smelting temperature is 550+/-10 ℃, the heating rate is 20 ℃ per minute, and the vacuum degree of the smelting furnace is less than 0.01Pa.
3. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (1), the holding time was 15 minutes.
4. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (3) or (4), the deformation amount of the extruded material at each extrusion is 3-5 mm.
5. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (3) or (4), the die is required to be insulated at 300 ℃ for 25-35 minutes in the extrusion process.
6. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (3) or (4), the extruded material is heated to 370-385 ℃ before extrusion.
7. The method for preparing the zinc-magnesium target according to claim 1, wherein the method comprises the following steps: in the step (5), machining is carried out at 525-625 RPM, and the feed rate is 0.08-0.12 mm/channel, so that the inner diameter, the outer diameter and the length of the target blank are machined until the outer oxide skin of the target is completely removed and the required dimensional tolerance is achieved.
8. The zinc-magnesium target is characterized in that: which is prepared by the preparation method of the zinc-magnesium target material according to any one of claims 1 to 7.
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| CN114481053B (en) * | 2022-01-25 | 2024-01-19 | 北京安泰六九新材料科技有限公司 | Magnesium zinc aluminum nickel vanadium alloy target and manufacturing method thereof |
| CN115122056A (en) * | 2022-08-01 | 2022-09-30 | 宁波江丰电子材料股份有限公司 | Processing method of evaporation material |
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